反应详情

温度

85 °C

A mixture of 105e (235 mg, 0.601 mmol), (4-fluoro-2-{6-oxo-8-thia-4,5-diazatricyclo[7.4.0.02,7]trideca-1(9),2(7),3-triene-5-yl}-6-(tetra-methyl-1,3,2-dioxaborolan-2-yl)phenyl)methyl acetate 108c (299 mg, 0.601 mmol), Pd(dppf)Cl2(42.8 mg, 0.06 mmol) and K3PO4(382 mg, 1.80 mmol) in ACN (10 mL) and H2O (2 mL) was degassed and stirred at 85° C. for 4 h under nitrogen. The reaction mixture was concentrated and the residue was purified by silica gel chromatography (EA/PE=4/1) to give N-[2-[[6-[[5-[5-fluoro-2-(acetoxymethyl)-3-(4-oxo-6,7,8,9-tetrahydrobenzothiopheno[2,3-d]pyridazin-3-yl)phenyl]-1-methyl-2-oxo-3-pyridyl]amino]-2-pyridyl]amino]ethyl]prop-2-enamide 105f (125 mg, 31%) as a brown solid. MS-ESI: [M+H]+ 684.3

1. customwas degassed
2. concentrationThe reaction mixture was concentrated
3. customthe residue was purified by silica gel chromatography (EA/PE=4/1)